CN114394588A - Method for continuously producing graphene by fluidized bed - Google Patents

Method for continuously producing graphene by fluidized bed Download PDF

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CN114394588A
CN114394588A CN202210122231.4A CN202210122231A CN114394588A CN 114394588 A CN114394588 A CN 114394588A CN 202210122231 A CN202210122231 A CN 202210122231A CN 114394588 A CN114394588 A CN 114394588A
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graphene
fluidized bed
gas
catalyst
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尉茂
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Wuhan Foresight Technology Co ltd
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    • C01B32/00—Carbon; Compounds thereof
    • C01B32/15—Nano-sized carbon materials
    • C01B32/182—Graphene
    • C01B32/184—Preparation
    • C01B32/186—Preparation by chemical vapour deposition [CVD]
    • C—CHEMISTRY; METALLURGY
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    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B2204/00—Structure or properties of graphene
    • C01B2204/04—Specific amount of layers or specific thickness
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B2204/00—Structure or properties of graphene
    • C01B2204/20—Graphene characterized by its properties
    • C01B2204/22—Electronic properties
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B2204/00—Structure or properties of graphene
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    • C01B2204/24—Thermal properties

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Abstract

The invention discloses a method for continuously producing graphene by a fluidized bed, which comprises the steps of placing a catalyst in a fluidized section, introducing inert gas, and blowing the catalyst to a fluidized state; and then starting the fluidized bed reactor for external heating, raising the temperature of the catalyst to 800-1000 ℃, continuously introducing carbon-containing gas into the reactor, introducing the product into an upper expansion section of the fluidized section, reducing the speed, separating graphene gas, and extracting the graphene gas from the top. According to the invention, the fluidized bed is adopted to continuously produce graphene, the fluidized catalyst is used as a matrix of vapor deposition, the deposition area of the carbon-containing gas is increased, the production efficiency is greatly increased, meanwhile, the catalysts collide with each other, and the separation of the generated graphene and the catalyst is realized by the speed reduction of the expansion section, so that the continuous production can be realized.

Description

Method for continuously producing graphene by fluidized bed
Technical Field
The invention relates to the technical field of graphene preparation, in particular to a method for continuously producing graphene by a fluidized bed.
Background
The CVD vapor deposition method is the best method for producing high-quality graphene at present, carbon-containing gas is introduced to a high-temperature copper foil in a closed environment, carbon atoms are decomposed at high temperature and orderly arranged on the surface of the copper foil to generate graphene, and the produced graphene has high quality, but has the defects of low efficiency, difficult product separation, high cost, incapability of large-scale production and the like. The existing large-scale production method is a redox method, has the problems of high cost, large pollution, many product defects and the like, and limits the development of the graphene industry.
Disclosure of Invention
The invention provides a method for continuously producing graphene by a fluidized bed, which solves the defects of the prior art, including but not limited to the defects.
In order to achieve the purpose, the scheme of the invention is as follows:
a method for continuously producing graphene by a fluidized bed comprises the following steps:
s1, placing a catalyst in a fluidization section, introducing inert gas, and blowing the catalyst to a fluidization state;
s2, starting the fluidized bed reactor to heat externally, raising the temperature of the catalyst to 800-1000 ℃, and continuously introducing carbon-containing gas;
and S3, the product enters an upper expansion section of the fluidization section to reduce the fluidization speed, and graphene gas is separated and extracted from the top.
In the invention, the fluidization speed of the catalyst is 50-70m/s, and the flow speed of the catalyst entering the upper expansion section of the fluidized bed reactor is 20-40 m/s.
In the invention, the catalyst is 20-60 meshes of copper powder or nickel powder.
In the invention, the carbon-containing gas is methane or natural gas, and the input amount is 2-10Nm3/h。
Further, at least one of ammonia gas and borane is doped into the carbon-containing gas.
Preferably, the molar ratio of the doping gas to the carbon-containing gas is 1 (5-10).
In the invention, the inert gas is nitrogen or argon.
In the invention, the inner diameter of the fluidization section is 0.2-0.4 m, and the height is 5-7 m; the inner diameter of the expansion section is 0.4-0.5 m.
In the invention, a gas distributor is arranged below the fluidization section according to the pressure of 400-600Nm3The amount of/h is 180m/s at a gas velocity of 150-.
Compared with the prior art, the invention has the beneficial effects that:
1. according to the invention, the fluidized bed is adopted to continuously produce graphene, the copper powder or nickel powder in a fluidized state is used as a matrix for vapor deposition creatively, the carbon-containing gas deposition area is increased, the production efficiency is greatly improved, meanwhile, the catalysts collide with each other, and the separation of the produced graphene and the catalysts is realized by the speed reduction of the expansion section, so that the continuous production can be realized.
2. According to the invention, ammonia gas or diborane gas is doped into carbon-containing gas, the ammonia gas and diborane have strong nitrogen and boron atom doping capability, the content of doping elements of the product is high, other impurity elements are not introduced, nitrogen-doped, boron-doped or nitrogen-boron double-doped graphene is generated, the doped nitrogen is in a negative charge state, the doped boron is in a positive charge state, and the electron energy band gap of the graphene is opened through doping, so that the electron current carrying capability, the conductivity and the heat conductivity are improved.
Drawings
FIG. 1 is a schematic view of a fluidized bed used in the production process of the present invention.
FIG. 2 is a scanning spectrum of an electron microscope for graphene obtained by the production method of the present invention.
FIG. 3 is an EDS energy spectrum of the graphene product obtained by the production method of the present invention.
Fig. 4 is a scanning microscope image of graphene prepared in comparative example 1 according to the present invention.
Fig. 5 is an electron microscope scanning spectrum of graphene prepared in comparative example 3 according to the present invention.
Labeled as: 1. a gas inlet; 2. a fluidizing section; 3. an expansion section; 4. a gas outlet; 21. a gas distributor; 22. and a heating coil.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
The invention provides a method for continuously producing graphene by a fluidized bed, which comprises the following steps:
1) putting 20-60 mesh copper powder or nickel powder serving as a catalyst into a fluidized bed reactor, replacing with inert gas such as nitrogen or argon, and keeping the micro-positive pressure of 50kPa in the reactor;
2) 400-600Nm3Speed per hourIntroducing inert gases such as nitrogen or argon into the fluidized bed reactor, spraying the gases into the fluidized bed through a gas distributor at a gas spraying speed of 150-180m/s, blowing the catalyst into a fluidized section to reach a fluidized state at a fluidizing speed of 50-70m/s, starting a heating coil outside the fluidized bed reactor, heating the catalyst at 120-160 kW, heating the catalyst by an induction magnetic field, and raising the temperature of the catalyst to 800-1000 ℃ and keeping the temperature;
3) continuously introducing methane or natural gas into the reactor, keeping the reaction temperature at 800-1000 ℃, carrying out vapor deposition on carbon-containing gas on the surface of the catalyst to generate graphene, separating the graphene and the catalyst by mutual collision in the fluidization process of the catalyst, falling the catalyst back to the fluidization section for continuous fluidization in an upper expansion section of the fluidized bed reactor as the gas flow rate is reduced to 20-40m/s, and extracting the graphene from the top of the fluidized bed reactor along with tail gas;
4) doping gases containing ammonia gas or borane and the like are doped into the reaction gases, so that nitrogen-doped graphene and boron-doped graphene can be synchronously generated.
The fluidized bed reactor used in the above production method is schematically shown in FIG. 1, and comprises a gas inlet 1 at the bottom, a fluidizing section 2 at the middle part, an expanding section 3 at the upper part and a gas outlet 4 at the top; the exterior of the fluidizing section 2 is provided with heating coils 22, and the inlet of the fluidizing section 2 is provided with a gas distributor 21, and the gas distributor 21 is used for controlling the distribution and velocity of the inlet gas, including the carbon-containing gas and the inert gas.
In the fluidized bed reactor, the inner diameter of the fluidized section 2 is 0.2-0.4 m, the height is 5-7m, the gas distributor 21 enables the gas spraying speed to reach 150-180m/s (working condition), the gas is uniformly sprayed to the fluidized section 2, the catalyst enters a fluidized state, and the fluidizing speed is 50-70 m/s; the heating coil 22 heats the catalyst through a magnetic field, and the heating power is 120-160 kW; the fluidization section 2 is made of 310S stainless steel, 304 stainless steel support rings, silicon steel magnet yokes, epoxy insulation plates, water copper coils, corundum refractory materials and silicon nitride wear-resistant layers from outside to inside; the inner diameter of the expanding section 3 is 0.4-0.5m, and the gas velocity of the catalyst can be reduced to 20-40m/s and falls back to the fluidizing section 2.
The invention uses the copper powder or nickel powder in a fluidized state as a matrix of vapor deposition, improves the deposition area of carbon-containing gas, greatly improves the production efficiency, simultaneously realizes the separation of the generated graphene and the catalyst by mutual collision between the catalysts and the reduction of the speed of an expansion section, can realize continuous production, and the content of the prepared graphene reaches 100 percent.
In various embodiments of the present invention, the amount of carbon-containing gas introduced is preferably controlled to be 2 to 10Nm3When the graphene is in a/h state, a scanning microscope image of the prepared graphene finished product is shown in fig. 2, so that the product is in a thin-layer sheet structure and has very good quality; an EDS energy spectrum chart is shown in FIG. 3, and the content of the prepared graphene reaches 100%.
In the invention, the doping gas is one or two of ammonia gas and diborane; the molar ratio of the doping gas to the carbon-containing gas is 1: (5-10). The ammonia gas and the diborane have strong nitrogen and boron atom doping capacity, the doping element content of the product is high, other impurity elements are not introduced, nitrogen-doped, boron-doped or nitrogen-boron double-doped graphene is generated, the doped nitrogen is in a negative charge state, the doped boron is in a positive charge state, the electronic energy band gap of the graphene is opened through doping, and the electronic current carrying capacity, the electric conductivity and the heat conductivity are improved.
Example 1
1) Placing 800kg of 40-mesh copper powder in a 2500L fluidized bed reactor, replacing nitrogen for 3 times until the oxygen content is lower than 10ppm, and keeping the pressure of the fluidized bed reactor at 50 kPa;
2) at 400Nm3Introducing nitrogen at a speed of/h, using copper powder to be in a fluidized state, wherein the fluidizing speed is 50m/s, starting the current of an external coil of the fluidized bed reactor, heating power is 140kW, and carrying out induction heating on the copper powder to 800 ℃;
3) continuously feeding 5Nm into the fluidized bed reactor3Methane, the fluidization speed of the expansion section is 20m/s, and the generated graphene is blown out of the reactor along with tail gas;
4) the graphene is collected, the number of obtained graphene layers is 3-5, the reaction rate of the product is 91%, and the content of the graphene reaches 100%.
Example 2
1) Placing 800kg of 60-mesh copper powder in a 2500L fluidized bed reactor, replacing nitrogen for 3 times until the oxygen content is lower than 10ppm, and keeping the pressure of the fluidized bed reactor at 50 kPa;
2) at 500Nm3Introducing nitrogen at a speed of/h, using copper powder to be in a fluidized state, wherein the fluidizing speed is 70m/s, starting the current of an external coil of the fluidized bed reactor, heating power is 140kW, and carrying out induction heating on the copper powder to 900 ℃;
3) continuously feeding 10Nm into the fluidized bed reactor3Methane, the fluidization speed of the expansion section is 40m/s, and the generated graphene is blown out of the reactor along with tail gas;
4) after the graphene is collected, the number of graphene layers is about 3-5, the reaction rate of the product is 90%, and the content of the graphene reaches 100%.
Example 3
1) Placing 800kg of 50-mesh nickel powder in a 2500L fluidized bed reactor, replacing nitrogen for 3 times until the oxygen content is lower than 10ppm, and keeping the pressure of the fluidized bed reactor at 50 kPa;
2) at 600Nm3Introducing nitrogen at a speed of/h, using nickel powder to be in a fluidized state, wherein the fluidizing speed is 60m/s, starting external coil current of the fluidized bed reactor, heating power is 140kW, and carrying out induction heating on the nickel powder to 900 ℃;
3) 2Nm continuous feed into the fluidized bed reactor3Methane, the fluidization speed of the expansion section is 28m/s, and the generated graphene is blown out of the reactor along with tail gas;
4) the graphene is collected, the number of obtained graphene layers is 3-5, the reaction rate of the product reaches 92%, and the content of the graphene reaches 100%.
Example 4
1) Placing 800kg of 20-mesh copper powder in a 2500L fluidized bed reactor, replacing for 3 times by nitrogen until the oxygen content is lower than 10ppm, and maintaining the pressure of the fluidized bed reactor at 50 kPa;
2) at 400Nm3Introducing nitrogen at a speed of/h, using copper powder to be in a fluidized state, wherein the fluidizing speed is 50m/s, starting the current of an external coil of the fluidized bed reactor, heating power is 140kW, and carrying out induction heating on the copper powder to 1000 ℃;
3) continuous feeding of 8Nm into the fluidized bed reactor3Introducing ammonia gas according to the mole ratio of 20% of methane into methane per hour, and blowing the generated graphene out of the reactor along with tail gas, wherein the fluidization speed of an expansion section is 22 m/s;
4) the graphene is collected, the number of obtained graphene layers is 3-5, the nitrogen doping amount is 9%, the product reaction rate reaches 92%, and the graphene content reaches 91%.
Example 5
1) Placing 800kg of 40-mesh copper powder in a 2500L fluidized bed reactor, replacing nitrogen for 3 times until the oxygen content is lower than 10ppm, and keeping the pressure of the fluidized bed reactor at 50 kPa;
2) at 500Nm3Introducing nitrogen at a speed of/h, using copper powder to be in a fluidized state, wherein the fluidizing speed is 56m/s, starting the current of an external coil of the fluidized bed reactor, heating power is 140kW, and carrying out induction heating on the copper powder to 900 ℃;
3) continuously feeding 5Nm into the fluidized bed reactor3Introducing ammonia gas according to the mole ratio of 20% of methane into methane per hour, and blowing the generated graphene out of the reactor along with tail gas, wherein the fluidization speed of an expansion section is 25 m/s;
4) the graphene is collected, the number of obtained graphene layers is 3-5, the reaction rate of the product is 91%, the nitrogen content is 9.1%, and the content of the graphene reaches 91.9%.
Example 6
1) Placing 800kg of 60-mesh copper powder in a 2500L fluidized bed reactor, replacing nitrogen for 3 times until the oxygen content is lower than 10ppm, and keeping the pressure of the fluidized bed reactor at 50 kPa;
2) at 600Nm3Introducing nitrogen at a speed of/h, using copper powder to be in a fluidized state, wherein the fluidizing speed is 70m/s, starting the current of an external coil of the fluidized bed reactor, heating power is 140kW, and carrying out induction heating on the copper powder to 900 ℃;
3) continuously feeding 5Nm into the fluidized bed reactor3Introducing diborane according to the mol ratio of 15% of methane into methane per hour, and blowing the generated graphene out of the reactor along with tail gas, wherein the fluidization speed of the expansion section is 36 m/s;
4) after the graphene is collected, the number of the graphene layers is 3-5, the boron doping amount is 3%, the product reaction rate is 92%, and the graphene content reaches 97%.
Example 7
1) Placing 800kg of 40-mesh nickel powder in a 2500L fluidized bed reactor, replacing nitrogen for 3 times until the oxygen content is lower than 10ppm, and keeping the pressure of the fluidized bed reactor at 50 kPa;
2) push button500Nm3Introducing nitrogen at a speed of/h, using nickel powder to be in a fluidized state, wherein the fluidizing speed is 52m/s, starting external coil current of the fluidized bed reactor, heating power is 140kW, and carrying out induction heating on the nickel powder to 900 ℃;
3) continuous feeding of 8Nm into the fluidized bed reactor3Introducing ammonia gas and 10% diborane according to the mole ratio of 10% of methane into methane, wherein the fluidization speed of an expansion section is 21m/s, and blowing the generated graphene out of the reactor along with tail gas;
4) the graphene is collected to obtain 3-5 layers of graphene, the reaction rate of the product is 90%, the nitrogen content is 9%, the boron content is 3%, and the graphene content is 88%.
Comparative example 1
The same procedure as in example 1, except that the induction heating temperature was maintained at 1050 ℃; after the graphene is collected, the number of graphene layers is 3-5, the reaction rate of the product is 91%, but a large number of carbon spheres are mixed in the graphene.
Comparative example 2
The same procedure as in example 1, except that the induction heating temperature was maintained at 750 ℃; after the graphene is collected, the number of the graphene layers is 3-5, the reaction rate of the product is 61%, and the reaction rate is lower.
Comparative example 3
The same procedure as in example 1, except that 50Nm of gas was continuously fed into the fluidized zone of the reactor3Methane, and blowing the generated graphene out of the reactor along with tail gas; after the graphene is collected, the number of the graphene layers is 20-30, and the reaction rate of the product is 90%.
Comparative example 4
The same procedure as in example 1, except that 0.5Nm of gas was continuously introduced into the fluidized zone of the reactor3Methane, and blowing the generated graphene out of the reactor along with tail gas; and after the graphene is collected, the graphene does not form a thin-layer sheet structure.
Comparative example 5
The method is the same as the method of the embodiment 5, except that ammonia gas is introduced according to the mole ratio of 30 percent of methane to generate graphene which is blown out of the reactor along with tail gas; after the graphene is collected, the number of the graphene layers is 3-5, the reaction rate of the product is 73%, and the reaction rate is lower.
Comparative example 6
The same procedure as in example 1 was followed, except that the fluidization velocity of the catalyst was controlled to 30m/s, the fluidization velocity of the expanded section was controlled to 20m/s, and the graphene having a significantly lamellar structure was not obtained by collection at the top of the column.
Comparative example 7
The same procedure as in example 1 was conducted except that the fluidization velocity of the catalyst was controlled to 80 m/s; the fluidization speed of the expansion section is 20m/s, the graphene does not form a thin-layer sheet structure after being collected at the top of the tower.
A microscopic scanning image of the finished graphene product prepared in the comparative example 1 is shown in fig. 4, and due to the fact that the reaction temperature is too high, secondary reaction occurs in tail gas, and a large number of carbon spheres are mixed in graphene; in comparative example 2, the reaction conversion rate is significantly reduced under the condition of lower reaction temperature; the graphene finished product prepared in comparative example 3 has a 20-30 layer structure due to the large amount of carbon-containing gas, and a microscopic scanning image is shown in fig. 5, so that the product is a relatively thick layer structure and is not an ideal thin-layer sheet; comparative example 4 in the case where the amount of the carbonaceous gas was relatively low, no lamellar structure was formed, which was associated with the collision of the catalyst in a fluidized state. In comparative example 5, when the doping gas was added in a large amount, the reaction conversion rate was significantly reduced, because it is likely that the vapor deposition was reduced due to an excessive amount of the doping gas. In the comparative example 6, under the condition that the fluidization speed of the catalyst is smaller, the mutual collision acting force between the catalysts is smaller, and the generated graphene is difficult to capture at the tower top; comparative example 7 in the case where the fluidization velocity was too large, there was a possibility that the collision force between the catalysts broke the lamellar sheet structure, resulting in non-molding of graphene.
Although embodiments of the present invention have been shown and described, it will be appreciated by those skilled in the art that changes, modifications, substitutions and alterations can be made in these embodiments without departing from the principles and spirit of the invention, the scope of which is defined in the appended claims and their equivalents.

Claims (9)

1. A method for continuously producing graphene by a fluidized bed is characterized by comprising the following steps:
s1, placing a catalyst in a fluidization section, introducing inert gas, and blowing the catalyst to a fluidization state;
s2, starting the fluidized bed reactor to heat externally, raising the temperature of the catalyst to 800-1000 ℃, and continuously introducing carbon-containing gas;
and S3, the product enters an upper expansion section of the fluidization section to reduce the fluidization speed, and graphene gas is separated and extracted from the top.
2. The method for continuously producing graphene by using the fluidized bed as claimed in claim 1, wherein the fluidization velocity of the catalyst is 50-70m/s, and the flow velocity of the catalyst entering the upper expansion section of the fluidized bed reactor is 20-40 m/s.
3. The method for continuously producing graphene by using the fluidized bed as claimed in claim 1, wherein the catalyst is 20-60 mesh copper powder or nickel powder.
4. The method for continuously producing graphene by using the fluidized bed as claimed in claim 1, wherein the carbon-containing gas is methane or natural gas, and the introduction amount is 2-10Nm3/h。
5. The method for continuously producing graphene by using the fluidized bed according to claim 4, wherein at least one of ammonia gas and borane is further doped into the carbon-containing gas.
6. The method for continuously producing graphene by using the fluidized bed as claimed in claim 5, wherein the molar ratio of the doping gas to the carbon-containing gas is 1 (5-10).
7. The fluidized bed continuous graphene production method according to claim 1, wherein the inert gas is nitrogen or argon.
8. The method for continuously producing graphene by using the fluidized bed as claimed in claim 1, wherein the inner diameter of the fluidized section is 0.2-0.4 m, and the height of the fluidized section is 5-7 m; the inner diameter of the expansion section is 0.4-0.5 m.
9. The method as claimed in claim 1, wherein a gas distributor is disposed below the fluidizing section and is 400-600Nm3The amount of/h is 180m/s at a gas velocity of 150-.
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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN116354340A (en) * 2023-03-14 2023-06-30 昆明理工大学 Low-cost large-scale preparation method of high-quality graphene
WO2023225438A1 (en) * 2022-05-20 2023-11-23 Clean Hydrogen Technologies Corp Systems and methods for pyrolysis reactions

Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102730673A (en) * 2012-07-04 2012-10-17 清华大学 Apparatus and method for continuously preparing thin-layer grapheme or hybrid combining thin-layer grapheme with thin-walled carbon nanotube
WO2013093358A1 (en) * 2011-12-22 2013-06-27 Arkema France Method for producing an assembly of carbon nanotubes and graphene
CN106219523A (en) * 2016-07-13 2016-12-14 清华大学 A kind of three dimensional network cage-shaped nano grapheme material and preparation method and application
CN106379885A (en) * 2016-08-31 2017-02-08 潍坊昊晟碳材料有限公司 Efficient preparation method of carbon nanotubes or graphene
CN106395794A (en) * 2016-08-31 2017-02-15 潍坊昊晟碳材料有限公司 Efficient continuous preparation method of coupled fluidized bed carbon nanotubes
CN207330368U (en) * 2017-09-29 2018-05-08 中山国安火炬科技发展有限公司 A kind of equipment with fluid bed production carbon nanotubes
CN111229026A (en) * 2020-02-11 2020-06-05 清华大学 Device and method for efficiently converting volatile organic compounds

Patent Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2013093358A1 (en) * 2011-12-22 2013-06-27 Arkema France Method for producing an assembly of carbon nanotubes and graphene
CN102730673A (en) * 2012-07-04 2012-10-17 清华大学 Apparatus and method for continuously preparing thin-layer grapheme or hybrid combining thin-layer grapheme with thin-walled carbon nanotube
CN106219523A (en) * 2016-07-13 2016-12-14 清华大学 A kind of three dimensional network cage-shaped nano grapheme material and preparation method and application
CN106379885A (en) * 2016-08-31 2017-02-08 潍坊昊晟碳材料有限公司 Efficient preparation method of carbon nanotubes or graphene
CN106395794A (en) * 2016-08-31 2017-02-15 潍坊昊晟碳材料有限公司 Efficient continuous preparation method of coupled fluidized bed carbon nanotubes
CN207330368U (en) * 2017-09-29 2018-05-08 中山国安火炬科技发展有限公司 A kind of equipment with fluid bed production carbon nanotubes
CN111229026A (en) * 2020-02-11 2020-06-05 清华大学 Device and method for efficiently converting volatile organic compounds

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
付长璟: "《石墨烯的制备、结构及应用》", 30 June 2017, 哈尔滨工业大学出版社, pages: 42 - 43 *

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2023225438A1 (en) * 2022-05-20 2023-11-23 Clean Hydrogen Technologies Corp Systems and methods for pyrolysis reactions
US12076718B2 (en) 2022-05-20 2024-09-03 Clean Hydrogen Technologies Corp Systems and methods for pyrolysis reactions
CN116354340A (en) * 2023-03-14 2023-06-30 昆明理工大学 Low-cost large-scale preparation method of high-quality graphene

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